HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 23316382, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 86740862 | HCID 86740862 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 23316382 | HCID 23316382 | 85% |
Reaction Steps
To chloroform (300 ml), 4-chloro-2-(4-chloro-α-hydroxybenzyl)-isonicotinanilide (12.4 g) and triethylamine (5.0 ml) were added. With stirring and under cooling with ice, phosphorus tribromide (9.1 g) was added slowly, and the stirring was continued for 1 hour. Following another 3-hour stirring at room temperature, the reaction mixture was poured into water. The chloroform layer was thoroughly washed with water and subsequently dried. The chloroform was completely distilled off under vacuum. Upon recrystallization from a mixed solvent of ethyl acetate and n-hexane, the titled compound was obtained in an amount of 10.1 g (yield: 85%). m.p. 140°-141° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04596801 |
| Source dataset | uspto-grants-1986_06 |
| ORD ID | ord-75301921d7ab4bba90cab30a240f9bb4 |
| Source note | uspto-grants-1986_06 |